CN107705980B - The preparation method of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer - Google Patents
The preparation method of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer Download PDFInfo
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- 230000005291 magnetic effect Effects 0.000 title claims abstract description 48
- 229910017061 Fe Co Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910002058 ternary alloy Inorganic materials 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000000151 deposition Methods 0.000 claims abstract description 26
- 230000008021 deposition Effects 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 15
- 239000010439 graphite Substances 0.000 claims abstract description 15
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 claims abstract description 13
- 239000003792 electrolyte Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004070 electrodeposition Methods 0.000 claims abstract description 8
- 230000001105 regulatory effect Effects 0.000 claims abstract description 7
- 238000004062 sedimentation Methods 0.000 claims abstract description 6
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 31
- 238000007254 oxidation reaction Methods 0.000 claims description 25
- 230000003647 oxidation Effects 0.000 claims description 21
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 12
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000002048 anodisation reaction Methods 0.000 claims description 5
- 238000005137 deposition process Methods 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- UYVVPOTVRSGDSX-UHFFFAOYSA-L [Cr](=O)(=O)(O)O.[P] Chemical compound [Cr](=O)(=O)(O)O.[P] UYVVPOTVRSGDSX-UHFFFAOYSA-L 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 239000011888 foil Substances 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000008139 complexing agent Substances 0.000 claims description 3
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 239000004471 Glycine Substances 0.000 claims description 2
- 230000003628 erosive effect Effects 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 244000025254 Cannabis sativa Species 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 239000002070 nanowire Substances 0.000 abstract description 45
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 abstract description 8
- 229910021577 Iron(II) chloride Inorganic materials 0.000 abstract description 8
- 229910017544 NdCl3 Inorganic materials 0.000 abstract description 8
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 abstract description 8
- 239000010408 film Substances 0.000 description 13
- 229910052761 rare earth metal Inorganic materials 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 150000002910 rare earth metals Chemical class 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000005030 aluminium foil Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
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- 238000005516 engineering process Methods 0.000 description 4
- 238000009415 formwork Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000005389 magnetism Effects 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000007743 anodising Methods 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000001808 coupling effect Effects 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 235000012149 noodles Nutrition 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- DWNBOPVKNPVNQG-LURJTMIESA-N (2s)-4-hydroxy-2-(propylamino)butanoic acid Chemical compound CCCN[C@H](C(O)=O)CCO DWNBOPVKNPVNQG-LURJTMIESA-N 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- KYAZRUPZRJALEP-UHFFFAOYSA-N bismuth manganese Chemical compound [Mn].[Bi] KYAZRUPZRJALEP-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- RIVZIMVWRDTIOQ-UHFFFAOYSA-N cobalt iron Chemical compound [Fe].[Co].[Co].[Co] RIVZIMVWRDTIOQ-UHFFFAOYSA-N 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000013598 vector Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/30—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates for applying nanostructures, e.g. by molecular beam epitaxy [MBE]
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
Abstract
A kind of preparation method of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer of the present invention.Method includes the following steps: (1) is by neodymium chloride (NdCl3·6H2O), frerrous chloride (FeCl2·4H2O), cobalt chloride (CoCl2·6H2O it) is mixed with deionized water, prepares NdxFeyCozLiquid is deposited, (2) then using graphite as anode, AAO template is cathode, using the deposition liquid of Nd-Fe-Co made from previous step as electrolyte, using D.C. regulated power supply, under the V DC voltage of 1.5 V ~ 2, carries out electrochemical deposition；Deposition current is the mA of 0.5 mA ~ 20, and sedimentation time is the h of 1 h ~ 2, finally obtains Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer.Gained number of nanowires of the invention is huge, and deposition is high.Nano wire is arranged in parallel, and high-sequential, line footpath is uniform, and draw ratio is very big.
Description
Technical field
Technical solution of the present invention is related to the magneto-optic memory technique containing rare earth metal and magnetic transition metal, specifically Nd-
The preparation method of Fe-Co ternary alloy three-partalloy magnetic nanometer.
Background technique
With the continuous development of information technology, information storage technology requires ultra high density and storage speed.Traditional magnetic
The packing density of recording medium is already close to superparamagnetic limit, while writing speed is limited develops slow with magnetization inversion speed
Slowly, therefore, seek ultra high density, the recording technique of superelevation storage speed have become current information technology field research heat
Point.
Magnetooptical memory material is that a kind of magnetic write-in light using Kerr magnetooptical effect reads out record, rewriting, deletes information
Carrier material.It has converged the advantages of optical storage and magnetic storage, and not only packing density with higher, writing speed also obtain
It improves.
Magnetooptical memory material mainly has following three kinds: manganese bismuth system alloy firm；Rare earth (RE)-transition metal (TM) amorphous
Film；Rare earth iron garnet.RE-TM noise is relatively high, and is easy to prepare large area uniform films on various substrates, is recent research
One of more magnetooptical memory material.
Nd-Fe-Co composite nano-line due to rare earth element and transition element Ferromagnetic coupling effect, it is with higher
Magnetocrystalline anisotropy, higher magnetic storage density, but storage speed is slow.Under the excitation of order vectors light field, light-magnetoelectricity is generated
Coupling effect, realize high speed magnetization inversion, to obtain ultrafast magnetic recording media.Currently, using magnetron sputtering technique preparation
TbFeCo, DyFeCo rare earth-transition race element thin film of amorphous alloy have obtained practical application as Magnetooptic recording medium.With
TbFeCo6For film, preparation process is as follows: rf magnetron sputtering is used on JGP560 type high vacuum magnetic control sputtering system
Method.Using ferrocobalt target as base target, substrate water cooling.Thin film composition is by Fe70Co30The number for the Tb item placed on composition target
And position is regulated and controled.The performance and uniformity of the recording medium film of this method preparation are strongly depend on sputtering power, target base
Away from, many factors such as gas pressure, back end vacuum degree.Affecting laws are also very complicated between these factors, thus target tissue and
Structural homogeneity superiority and inferiority also will finally influence quality of forming film by sputtering mode.Sputtering power will affect the internal structure of film with
Thermal stress；The variation of sputtering pressure will affect the generation and its optical property of film, see [Guo Jihua, Huang Zhixin, Cui Zengli, poplar
It is of heap of stone, Shao Jianbo, Zhu Hongsheng, influence [J] the functional material of Zhang Ping sputtering technology to GdTbFeCo film magneto-optical property, 2009,
11(40):1802-1804.]。
Summary of the invention
It is an object of the present invention to for deficiency present in current techniques, provide a kind of Nd-Fe-Co ternary alloy three-partalloy magnetism to receive
The preparation method of rice noodles.The patent has been put forward for the first time the side that NdFeCo alloy firm is prepared for using direct current electrochemical deposition method
Method, and the ion concentration of light rare earth Nd element is had adjusted, the Nd-Fe-Co ternary alloy three-partalloy magnetism for being prepared for heterogeneity for the first time is received
Nanowire arrays.It joined heavy rare earth Nd element in the composition of the composite magnetic nano wire, Nd element is right as ideal pinning phase
Neticdomain wall generates pinning mechanism, optimizes crystallite dimension micro-structure, improves the magnetic property of nano wire.Thus make Nd-Fe-Co tri-
First alloy nano-wire becomes the magneto-optic memory technique with preferable magnetic energy product.Present invention process process is simple, and controllability is strong, and preparation is received
Nanowire arrays uniformity is good and high-sequential.
The technical scheme is that
A kind of preparation method of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer, comprising the following steps:
(1) configures NdxFeyCozDeposit liquid
By neodymium chloride (NdCl3·6H2O), frerrous chloride (FeCl2·4H2O), cobalt chloride (CoCl2·6H2) and deionization O
Water mixing, prepares NdxFeyCozLiquid is deposited, atomic percent is calculated as Nd:Fe:Co=2~16:7~15:1~2；It additionally incorporates sweet
Propylhomoserin (NH2CH2COOH), boric acid (H3BO3) and ascorbic acid (C6H8O6) it is used as complexing agent；Wherein, each ingredient in liquid is deposited
Concentration is respectively as follows: C (NdCl3·6H2O)=0.1~0.8mol/L, C (FeCl2·4H2O)=0.35~0.75mol/L, C
(CoCl2·6H2O)=0.05~0.1mol/L, C (H3BO3)=0.48mol/L, C (C2H5NO2)=0.2mol/L, C (C6H8O6)
=0.023mol/L；
(2) deposition of .Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer
Using graphite as anode, AAO template is cathode, using the deposition liquid of Nd-Fe-Co made from previous step as electrolyte, is utilized
D.C. regulated power supply carries out electrochemical deposition under 1.5V~2V DC voltage；Deposition current is 0.5mA~20mA, when deposition
Between be 1h~2h, finally obtain Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer；
The deposition process carries out on magnetic stirring apparatus, and revolving speed is 1r/s~5r/s.；
The preparation method of the AAO template, preferably comprises following steps:
(1) aluminium flake pre-processes
Purity will be cut to required size for 99.999% high-purity aluminum foil, then using annealing, cleaning and throwing
Light completes pretreatment；
Wherein, annealing temperature is 500 DEG C, annealing time 5h；
Polishing treatment: electrolyte is made with dehydrated alcohol and the perchloric acid solution that 4:1 is prepared by volume, yin is made with graphite
Pole, aluminium foil make anode, polish 5min under 15V voltage；
(2) two-step anodization
It aoxidizes for the first time: being anode by the aluminium flake after polishing treatment, using graphite as cathode, electrolyte selects 0.3mol/L's
Oxalic acid solution, steady state voltage 40V, oxidization time 4h；Then 4h is reacted in 60 DEG C of phosphorus chromic acid solution after aluminium flake being taken out；
Second of oxidation is carried out again: being anode by the aluminium flake by oxidation for the first time, and using graphite as cathode, electrolyte is selected
The oxalic acid solution of 0.3mol/L；
(3) bottom is gone to
CuCl will be saturated2Solution drop is in a side surface of the aluminium flake by two-step anodization, after reacting 1min~2min
Erosion is washed away with deionized water, manifests pellumina transparent in the middle part of template；
(4) reaming
Aluminium flake that upper step obtains is impregnated into 1h in 30 DEG C, the phosphoric acid solution of 5wt% again；
(5) metal spraying
When being evacuated to air pressure and being down to 10Pa~1Pa, aluminium flake metal spraying that step (4) is obtained；Metal spraying process starts, the time
It is adjusted to 5min, current control is between 10mA~20mA, and it is quiet to 3min~5min after the completion of metal spraying process, obtain AAO template.
It carries out in the vacuum tube furnace being annealed under argon atmosphere protective condition in the step (1), is needed before use
It is evacuated to 10Pa~100Pa.
The beneficial effects of the present invention are: heavy rare earth Nd element is added in Fe-Co deposition liquid by the method for the present invention, it is prepared for
NdxFeyCozTernary deposits liquid, and Nd-Fe-Co composite magnetic nano wire has been made by direct current electrochemical deposition.Gained nano wire
Enormous amount, deposition are high.Nano wire is arranged in parallel, and high-sequential, line footpath is uniform, and draw ratio is very big.Nd element is to neticdomain wall
Pinning mechanism is generated, grain microstructure is optimized, improves the coercivity of nano wire.The coercivity of the nano wire up to 620Oe,
Saturation magnetization reaches 30.54emu/g.More specifically, beneficial effects of the present invention and its mechanism are as follows:
(1) by two-step electrochemical anodizing method prepare alumina formwork high-sequential, duct is arranged in parallel, and all vertically with
Template surface growth.Template channel diameter is 50nm~60nm, and major diameter is bigger.Nano wire is under the supporting role of template, limit
Domain growth, size is uniform, neat and orderly.
(2) the method for the present invention makees anode with graphite, and homemade alumina formwork makees cathode, by direct current electrochemical deposition,
The Nd in liquid will be deposited3+、Fe2+、Co3+It is reduced to metallic atom, under electrical field draw, is grown in template congregate.Deposition
Before, it needs in one layer of golden film of template base injcction, to increase template electric conductivity.Deposition process voltage control 1.5V~2V it
Between, electric current is no more than 20mA.Because electric current is excessive, deposition rate is easy very much blocking hole fastly, forms nanometer thin in template surface
Film is unable to get the nano-wire array of rule.
(3) the Nd-Fe-Co composite magnetic nanowire deposition rate of the method for the present invention preparation is high, and nanowire alignment is regular,
Enormous amount.Heavy rare earth Nd element generates pinning effect to neticdomain wall, is that magnetic domain deflection is difficult, anisotropy field enhancing, coercive
Power increases, and can be used as good magnetooptical memory material.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the oxidation unit figure of anodised aluminium (AAO) template.
Fig. 2 is the field emission scanning electron microscope photo of alumina formwork, wherein Fig. 2 (a) is front elevation；Fig. 2 (b) is Fig. 2 a
The enlarged drawing of middle region (1).
Fig. 3 is the schematic device that magnetic nanometer carries out electrochemical deposition.
Fig. 4 be embodiment 4 made from Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer FESEM map wherein, Fig. 4 (a) is
Front elevation；Fig. 4 b) it is side view.
The EDS map of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer made from Fig. 5 embodiment 4.
Wherein, Fig. 6 (a) is the transmission electron microscope photo of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer made from Fig. 6 embodiment 4
Nanocluster；Fig. 6 (b) is single nano-wire high-resolution photo.
Wherein for Nd-Fe-Co ternary alloy nano line hysteresis loop made from embodiment 4, Fig. 7 (a) is deposited to Fig. 7；
Fig. 7 (b) is 660 DEG C of annealing 3h.
Specific embodiment
Embodiment 1
Step 1: the preparation of AAO template
The preparation of nano wire is carried out using AAO template herein.AAO template be use purity for 99.999%, with a thickness of
What 0.3mm high-purity aluminum foil was prepared in oxalic acid solution by two-step electrochemical anodizing method.It mainly include aluminium flake pretreatment, secondary sun
The several processes in barrier layer are gone in pole oxidation, removal aluminium substrate, reaming.
(1) aluminium flake pre-processes
It cuts out: aluminium foil is cut to the sequin of diameter 20mm, be close to the diameter of washer used when oxidation.
Annealing: then making annealing treatment aluminium flake in the vacuum tube furnace under argon atmosphere protective condition, annealing temperature
Degree is 500 DEG C, and annealing time is set as 5h, cools to room temperature with the furnace after annealing.
It develops a film: aluminium flake is successively utilized respectively in acetone, dehydrated alcohol to ultrasonic washing instrument oscillation cleaning 5min.It will be through
It crosses aluminium flake of developing a film that treated and is put into the NaOH solution of 10wt% and impregnate 15min or so, to remove aluminium foil surface oxide layer.
Polishing treatment: with dehydrated alcohol and perchloric acid, (dehydrated alcohol and perchloric acid are all analytical reagents, and dehydrated alcohol is dense
Degree be 99.99%, perchloric acid concentration be 70%~72%) by volume 4:1 prepare solution make electrolyte, with graphite make yin
Pole, aluminium foil make anode, polish 5min under the voltage of 15V or so.Burnishing device is known device, by D.C. regulated power supply, stone
Electrode ink, aluminium flake, polishing fluid (being placed in beaker) are formed by connecting.
(2) two-step anodization
Once oxidation: carrying out once oxidation for the aluminium flake after polishing treatment, and using graphite as cathode, aluminium flake is anode, electrolysis
The oxalic acid solution of liquid selection 0.3mol/L.Steady state voltage is 40V, oxidization time 4h.Electrolytic cell will be placed on ice water in oxidation process
In the environment of mixture, room temperature is maintained at 17 DEG C.Fig. 1 is the oxidation unit schematic diagram of AAO template, which is this field
Known device, main group become D.C. regulated power supply, ammeter, electrolytic cell (or being dislodger), conducting wire, graphite electrode and (do sun
Pole).Those skilled in the art install equipment according to Fig. 1, can carry out oxidation operation.
Descale: since the oxide skin degree of order obtained by once oxidation is poor, the oxide skin of once oxidation is removed.Tool
Gymnastics conduct: in deionized water, phosphorus chromic acid solution needed for configuring descale, phosphoric acid and chromic acid concentration are respectively in solution
0.2wt% and 0.1wt%.AAO template is placed in phosphorus chromic acid solution, reacts 4h in 60 DEG C of water-baths.
Carry out secondary oxidation again: other reaction conditions of secondary oxidation are identical as once oxidation, and oxidization time is then extended for
6h.The resulting oxidation film high-sequential of secondary oxidation, quality is preferable, therefore carries out subsequent system using the template after secondary oxidation
It is standby.
(3) bottom is gone to
CuCl will be saturated2Solution drop is allowed to react with aluminium base at the back side of the aluminium flake by second of oxidation.React 1min
~2min washes away the metallic monolith object eroded with deionized water, only pellumina transparent in the middle part of remaining template.
(4) reaming
The phosphoric acid solution for selecting 5wt% handles 1h under 30 DEG C of waters bath with thermostatic control.
(5) metal spraying
When being evacuated to air pressure and being down to 10Pa~1Pa, start metal spraying.Metal spraying process starts, and the time is adjusted to 5min, electric current control
System is between 10mA~20mA, quiet to 3min~5min after the completion of metal spraying process, etc. air pressure insides and temperature stablize after open again
Instrument takes out AAO template.Fig. 2 is the field emission scanning electron microscope photo of AAO template.Fig. 2 a is the front elevation of template, and Fig. 2 b is figure
The enlarged drawing of region (1) in 2a.By can see in figure, the AAO template surface of preparation is smooth, and hole is uniformly and height has
Sequence is measured pore size and is consistent substantially, is 50nm~60nm, pitch of holes is about 100nm.Nano aperture all becomes substantially
It is bordering on circle, arrangement is uniform.Substantially 60 ° of the geometrical orientation difference of adjacent holes.
Step 2: configuration Nd-Fe-Co deposits liquid
By neodymium chloride (NdCl3·6H2O), frerrous chloride (FeCl2·4H2O), cobalt chloride (CoCl2·6H2) and deionization O
Water (avoids introducing foreign ion) mixing, and preparation obtains Nd-Fe-Co deposition liquid.Glycine is added by fixed mixing ratio simultaneously
(NH2CH2COOH), boric acid (H3BO3) and ascorbic acid (C6H8O6) it is used as complexing agent, the pH value of solution is 2.0~3.0 at this time,
Deposition voltage is maintained at 1.5V, and such solution can improve inoxidizability, the electric conductivity of deposition liquid simultaneously.Each ingredient in solution
Concentration range be respectively as follows: C (NdCl3·6H2O)=0.1mol/L, C (FeCl2·4H2O)=0.75mol/L, C (CoCl2·
6H2O)=0.1mol/L, C (H3BO3)=0.48mol/L, C (C2H5NO2)=0.2mol/L, C (C6H8O6)=0.023mol/L.
Step 3: the deposition of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer
In the precipitation equipment of such as Fig. 3, using graphite as anode, AAO template made from the first step is cathode, in 1.5V direct current
Under voltage, electrochemical deposition is carried out, deposition current is maintained at 0.5mA~20mA, sedimentation time 2h.Deposition process is stirred in magnetic force
It mixes and is carried out on device, revolving speed is 1r/s~5r/s, accelerates effects of ion diffusion, makes to deposit each section ion concentration basic one in liquid
It causes, further improves gained Nanowire Quality.The device device of Fig. 3 is equipment known in this field, D.C. regulated power supply, ampere
Table, electrolytic cell (or being dislodger), conducting wire, graphite electrode (doing anode), constant temperature Bidirectional magnetic agitator.Those skilled in the art according to
Equipment is installed shown in Fig. 3, deposition operation can be carried out.
Metallic atom ratio is Tb:Fe:Co=2:15:2 in the present embodiment, and mass ratio is about 5:22:4.
Embodiment 2
Constituent concentration each in embodiment 1 is changed to C (NdCl3·6H2O)=0.1mol/L, C (FeCl2·4H2O)=
0.35mol/L, C (CoCl2·6H2O)=0.1mol/L, C (H3BO3)=0.48mol/L, C (C2H5NO2)=0.2mol/L, C
(C6H8O6)=0.023mol/L, other are the same as embodiment 1.
Metallic atom ratio is Tb:Fe:Co=2:7:2 in the present embodiment, and mass ratio is about 5:10:4.
Embodiment 3
Constituent concentration each in embodiment 1 is changed to C (NdCl3·6H2O)=0.4mol/L, C (FeCl2·4H2O)=
0.35mol/L, C (CoCl2·6H2O)=0.05mol/L, C (H3BO3)=0.48mol/L, C (C2H5NO2)=0.2mol/L, C
(C6H8O6)=0.023mol/L, deposition voltage are changed to 2V, and sedimentation time is changed to 1h, other are the same as embodiment 1.
Metallic atom ratio is Tb:Fe:Co=8:7:1 in the present embodiment, and mass ratio is about 4:5:1.
Embodiment 4
Constituent concentration each in embodiment 1 is changed to C (NdCl3·6H2O)=0.8mol/L, C (FeCl2·4H2O)=
0.35mol/L, C (CoCl2·6H2O)=0.05mol/L, C (H3BO3)=0.48mol/L, C (C2H5NO2)=0.2mol/L, C
(C6H8O6)=0.023mol/L, deposition voltage are changed to 2V, and sedimentation time is changed to 1h, other are the same as embodiment 1.
Metallic atom ratio is Tb:Fe:Co=16:7:1 in the present embodiment, and mass ratio is about 8:5:1.
Fig. 4 is scanning of the Nd-Fe-Co magnetic nanometer made from embodiment 4 after the dissociation of the NaOH solution part of 5wt%
Electromicroscopic photograph, wherein Fig. 4 a is nano wire front shape appearance figure, the enlarged drawing of Fig. 4 b front scan image.It can see by Fig. 4 a,
Nanowire growth is intensive, and filling rate is very high, and the hole of AAO template is nearly all filled.Lodging is presented in nano wire distribution at random
Phenomenon, this is because sodium hydroxide dissociation, decomposes alumina formwork, nano wire loses backing material.By in Fig. 4 b
It can be seen that nanowire length is up to 20 microns.
It is formed in order to further determine the element of gained nano wire, ingredient point is carried out to nano wire using X-ray energy spectrometer
Analysis.Fig. 5 is the EDS map of Nd-Fe-Co magnetic nanometer made from embodiment 4, lists nanometer in the table in the upper right corner in figure
The constituent and atomic ratio of line.Nd, Fe and Co are the components of nano wire, this explanation, transition element Fe, Co are successfully lured
It is derived heavy rare earth element Nd, co-deposition phenomenon has occurred, successfully prepares Nd-Fe-Co nano wire.Meanwhile nano wire is received
Each element does quantitative analysis discovery in rice noodles, and in Nd-Fe-Co alloy nano-wire, Nd:Fe:Co atomic ratio is 4:15:2, Nd's
Deposition is considerably less.This is mainly due to the sedimentation potential of Nd is too negative, differ greatly with transition element, during the deposition process,
Fe2+、Co2+Induce Nd3+It deposits extremely difficult.
Fig. 6 is the TEM photo of Nd-Fe-Co magnetic nanometer made from embodiment 4.Fig. 6 a is the shape appearance figure of nano wire bundle,
By can see in figure, the uniform diameter of nano wire is consistent, does not dissociate complete AAO template and is sticked together, and forms nano wire
Beam.Part nano wire is different in size in figure, this is because using at ultrasonic oscillation dispersion when preparing transmission electron microscope sample
Reason, part nano wire are interrupted.Obtaining nanowire diameter with Ruler software measurement is about 50nm.Fig. 6 a is the high score of nano wire
Distinguish lattice photo.Faint lattice phase as we can see from the figure illustrates that deposited Nd-Fe-Co magnetic nanometer is microstructure.
Fig. 7 is the hysteresis loop of the annealing of Nd-Fe-Co magnetic nanometer made from embodiment 4 front and back.Tables 1 and 2 lists implementation respectively
The magnetic property data of parallel, the vertical outer magnetic field direction of 4 gained nano-wire array of example.From the figure, it can be seen that either deposited
Or annealed state, the magnetic property that nano wire is parallel to outer magnetic field direction be always better than nano wire vertically with the magnetism of outer magnetic field direction
Can, this is caused by the shape anisotropy of nano wire.Comparison diagram 7a and Fig. 7 b can see, after 660 DEG C of annealing 3h, nano wire
Coercivity is obviously improved, this is because deposited nano wire is microstructure, is changed into polycrystalline structure, coercive after annealing
Power enhancing.Meanwhile rare earth element nd generates pinning effect to neticdomain wall, enhances anisotropy field, magnetic property gets a promotion.
Table 1 is that external magnetic field is parallel to the magnetic property data on nano wire direction.
Table 2 is external magnetic field perpendicular to the magnetic property data on nano wire direction.
Unaccomplished matter of the present invention is well-known technique.
Claims (4)
1. a kind of preparation method of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer, it is characterized in that method includes the following steps:
(1) Nd is configuredxFeyCozDeposit liquid
Neodymium chloride, frerrous chloride, cobalt chloride and deionized water are mixed, Nd is preparedxFeyCozDeposit liquid, atomic percent are as follows:
Nd:Fe:Co=2~16:7~15:1~2；Additionally incorporate glycine (NH2CH2COOH), boric acid (H3BO3) and ascorbic acid (C6H8O6)
As complexing agent；Wherein, the concentration for depositing each ingredient in liquid is respectively as follows: C (neodymium chloride)=0.1 ~ 0.8 mol/L, C (protochloride
Iron)=0.35 ~ 0.75 mol/L, C (cobalt chloride)=0.05 ~ 0.1 mol/L, C (H3BO3)=0.48 mol/L, C (C2H5NO2)=
0.2 mol/L, C (C6H8O6)=0.023 mol/L；
(2) deposition of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer
Using graphite as anode, AAO template is cathode, using the deposition liquid of Nd-Fe-Co made from previous step as electrolyte, utilizes direct current
Regulated power supply carries out electrochemical deposition under the V DC voltage of 1.5 V ~ 2；Deposition current is the mA of 0.5 mA ~ 20, sedimentation time
For the h of 1 h ~ 2, Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer is finally obtained.
2. the preparation method of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer as described in claim 1, it is characterized in that the step
Suddenly deposition process carries out on magnetic stirring apparatus in (2), and revolving speed is the r/s of 1 r/s ~ 5.
3. the preparation method of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer as described in claim 1, it is characterized in that the AAO
The preparation method of template, includes the following steps:
(1) aluminium flake pre-processes
Purity will be cut to required size for 99.999% high-purity aluminum foil, it is complete then using annealing, cleaning and polishing
At pretreatment；
Wherein, annealing temperature is 500 DEG C, and annealing time is 5 h；
Polishing treatment: electrolyte is made with dehydrated alcohol and the perchloric acid solution that 4:1 is prepared by volume, cathode, aluminium are made with graphite
Foil makees anode, polishes 5 min under 15 V voltages；
(2) two-step anodization
It aoxidizes for the first time: being anode by the aluminium flake after polishing treatment, using graphite as cathode, electrolyte selects the grass of 0.3 mol/L
Acid solution, steady state voltage are 40 V, 4 h of oxidization time；Then 4 are reacted in 60 DEG C of phosphorus chromic acid solution after aluminium flake being taken out
h；
Second of oxidation is carried out again: being anode by the aluminium flake by oxidation for the first time, and using graphite as cathode, electrolyte selects 0.3
The oxalic acid solution of mol/L；
(3) bottom is gone to
CuCl will be saturated2Solution drop is spent after reacting the min of 1min ~ 2 in a side surface of the aluminium flake by two-step anodization
Ionized water washes away erosion, manifests pellumina transparent in the middle part of template；
(4) reaming
Aluminium flake that upper step obtains is impregnated into 1 h in 30 DEG C, the phosphoric acid solution of 5 wt% again；
(5) metal spraying
When being evacuated to air pressure and being down to 10 Pa ~ 1 Pa, aluminium flake metal spraying that step (4) is obtained；Metal spraying process starts, time tune
To 5 min, current control is between the mA of 10 mA ~ 20, quiet to the min of 3 min ~ 5 after the completion of metal spraying process, obtains AAO template.
4. the preparation method of Nd-Fe-Co ternary alloy three-partalloy magnetic nanometer as claimed in claim 3, it is characterized in that the step
Suddenly it is carried out in the vacuum tube furnace being annealed under argon atmosphere protective condition in the pretreatment of (1) aluminium flake, needs to vacuumize before use
To the Pa of 10Pa ~ 100.
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